CN116080033A - Preparation method of multilayer co-extrusion bioreactor membrane material - Google Patents
Preparation method of multilayer co-extrusion bioreactor membrane material Download PDFInfo
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- CN116080033A CN116080033A CN202310108030.3A CN202310108030A CN116080033A CN 116080033 A CN116080033 A CN 116080033A CN 202310108030 A CN202310108030 A CN 202310108030A CN 116080033 A CN116080033 A CN 116080033A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
- B29C48/16—Articles comprising two or more components, e.g. co-extruded layers
- B29C48/18—Articles comprising two or more components, e.g. co-extruded layers the components being layers
- B29C48/21—Articles comprising two or more components, e.g. co-extruded layers the components being layers the layers being joined at their surfaces
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
- B29C48/001—Combinations of extrusion moulding with other shaping operations
- B29C48/0018—Combinations of extrusion moulding with other shaping operations combined with shaping by orienting, stretching or shrinking, e.g. film blowing
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
- B29C48/001—Combinations of extrusion moulding with other shaping operations
- B29C48/0021—Combinations of extrusion moulding with other shaping operations combined with joining, lining or laminating
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
- B29C48/25—Component parts, details or accessories; Auxiliary operations
- B29C48/28—Storing of extruded material, e.g. by winding up or stacking
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
- B29C48/25—Component parts, details or accessories; Auxiliary operations
- B29C48/88—Thermal treatment of the stream of extruded material, e.g. cooling
- B29C48/885—External treatment, e.g. by using air rings for cooling tubular films
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29L—INDEXING SCHEME ASSOCIATED WITH SUBCLASS B29C, RELATING TO PARTICULAR ARTICLES
- B29L2007/00—Flat articles, e.g. films or sheets
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29L—INDEXING SCHEME ASSOCIATED WITH SUBCLASS B29C, RELATING TO PARTICULAR ARTICLES
- B29L2009/00—Layered products
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W10/00—Technologies for wastewater treatment
- Y02W10/10—Biological treatment of water, waste water, or sewage
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Abstract
The invention discloses a preparation method of a multilayer co-extrusion bioreactor membrane material, which comprises the following steps: s1, heating and melting extrusion of a film material through a multilayer coextrusion device, and conveying the film material to a stretching traction roller in a stretching system; s2, conveying the film material through a traction roller, performing preliminary cooling by a cooling roller, and shaping; s3, carrying out secondary heating on the liquid contact layer through infrared radiation heating equipment to form a semi-molten state, and carrying out electrostatic spraying on the liquid contact layer with nano particles; s4, performing secondary lamination on the film through a second group of cooling rollers. The invention adopts a multilayer coextrusion casting extrusion process, and performs electrostatic spraying on the liquid contact layer of the membrane material to cover the surface with a layer of fumed silica, and a great amount of experiments prove that the membrane material has higher cell culture effect. The multilayer co-extrusion bioreactor membrane material has better biocompatibility, higher gas barrier property and high bending resistance and puncture resistance.
Description
Technical Field
The invention relates to the technical field of bioreactor production and manufacturing, in particular to a preparation method of a multilayer co-extrusion bioreactor membrane material.
Background
In the biopharmaceutical production, disposable bags are gaining acceptance worldwide and gradually replacing the traditional reusable stainless steel systems. Because the reactor and the incubator, the price of the transfer device is high, the cleaning after the use is difficult, the stainless steel system occupies a large area, and the transfer is inconvenient.
The disposable biological process bag adopts advanced sterilization and disinfection, is convenient to use, and can improve the working efficiency. The floor area is small, the step of cleaning the reactor in the production process can be reduced, and the uncertainty of cross infection in use is avoided.
In the prior art, a multilayer coextrusion blow molding mode is mostly adopted to produce films, the films are extruded through a coextrusion die head, and the films are pulled and coiled after air cooling and water cooling. An increase in the thickness of the co-extrusion blown film results in a decrease in transparency, which is detrimental to the observation of cell growth. Wherein the barrier property, tensile strength and cell culture density of the film are lower than those of the co-extrusion casting film.
Disclosure of Invention
The present invention aims to provide a method for preparing a multilayer co-extrusion bioreactor membrane material, which solves one or more of the above-mentioned problems in the prior art.
The invention provides a preparation method of a multilayer co-extrusion bioreactor membrane material, which comprises the following steps:
s1, heating and melting extrusion of a film material through a multilayer coextrusion device, and conveying the film material to a stretching traction roller in a stretching system;
s2, conveying the film material through a traction roller, performing preliminary cooling by a cooling roller, and shaping;
s3, carrying out secondary heating on the liquid contact layer through infrared radiation heating equipment to form a semi-molten state, and carrying out electrostatic spraying on the liquid contact layer with nano particles;
s4, performing secondary lamination on the film through a second group of cooling rollers.
In certain embodiments, in step S1, the multilayer coextrusion device is preheated to a temperature of 120-240℃for a period of 30-90 minutes; the temperature of the die head is 200-250 ℃; the temperature of the feed inlet is 80-150 ℃, so that the particles can be conveniently conveyed.
In certain embodiments, in step S1, the film material includes, in order from outside to inside, a protective layer, an adhesive layer, a gas barrier layer, an adhesive layer, and a liquid contact layer;
the protective layer is composed of mixed resin of linear low-density polyethylene and metallocene polyethylene, the thickness of the protective layer is 50-80 mu m, the mass ratio of the linear low-density polyethylene is 60-90%, and the mass ratio of the metallocene polyethylene is 10-40%; the adhesive layer is made of ethylene-vinyl acetate copolymer, the thickness of the adhesive layer is 10-18 mu m, and the melt extrusion temperature is 160-200 ℃; the gas barrier layer is made of ethylene-vinyl alcohol copolymer, and the thickness of the gas barrier layer is 20-60 mu m; the liquid contact layer is made of metallocene polyethylene and linear low-density polyethylene, the thickness of the liquid contact layer is 150-250 mu m, the mass ratio of the metallocene polyethylene is 10-40%, and the mass ratio of the linear low-density polyethylene is 60-90%.
Wherein: the thickness of the bonding layer is not required to be too thick, and the functional layer is only required to be well combined;
the gas barrier layer is made of ethylene-vinyl alcohol copolymer (EVOH), and the EVOH has good air permeability, high transparency and good glossiness, and can more intuitively see the cell growth;
the liquid contact layer adopts metallocene polyethylene and linear low density polyethylene as raw materials, and controls the mass ratio of the metallocene polyethylene and the linear low density polyethylene, so that the cell growth can be better promoted, and low molecular substances cannot be separated out in the use process, so that the normal growth of cells is affected.
In certain embodiments, further comprising performing a thickness test on the extruded film, comprising the steps of:
the film was stretched and an infrared image was obtained and the thickness of each edge was tested.
Wherein: in the process of testing the edge thickness, the die head is finely adjusted at the place with uneven thickness, or the rotating speed of the traction roller is reduced, the stretching force of the film is reduced, and the thickness of the film material is timely adjusted.
The stretching system comprises a plurality of groups of traction rollers which are arranged side by side in the same direction, the rotating speed frequency of the second group of traction rollers is 1-1.2 times faster than that of the first group of traction rollers, the film material is conveyed through an infrared thermal imager image among the groups of traction rollers, the flatness of the film material is observed, and the position with uneven thickness is finely adjusted.
In certain embodiments, in step S2, the cooling temperature of the first set of cooling rolls is 60-150 ℃. And (3) performing preliminary cooling shaping on the membrane material, and preparing for post-treatment processing.
In certain embodiments, in step S3, the surface of the liquid contact layer is heated by an infrared radiation heating device to a semi-molten state, the heating temperature is between Tm-Tf of the liquid contact layer, and the surface is subjected to electrostatic powder spraying of fumed silica by an electrostatic spraying device, so that the fumed silica adheres firmly to the surface of the metallocene polyethylene.
Specifically, the heating temperature is 120-180 ℃. Through the electrostatic spraying, the problems of uneven dispersion, easy agglomeration, blockage of a spray gun and the like in the powder spraying process can be solved.
Wherein: by adding an appropriate amount of fumed silica (SiO 2 ) The transparency, the strength, the toughness, the waterproof performance and the ageing resistance are not affected, the strength, the toughness, the waterproof performance and the ageing resistance are also obviously improved, and the biological cell culture is also better affected.
In certain embodiments, in step S3, the nanoparticles are prepared by mixing fumed silica and a dispersant in proportions;
wherein: the particle size of the fumed silica is 0.02 μm; the dispersing agent is selected from polymethacrylic acid, and the mass ratio of the dispersing agent is controlled to be 0.8%.
In certain embodiments, instead of fumed silica, several of the following may also be used to increase the rate of cell growth, such as calcium phosphate (Ca 3 (PO 4 ) 2 ) Calcium carbonate (CaCO) 3 ) Calcium sulfate (CaSO) 4 ) Calcium silicate (CaSiO) 4 ) Etc.
In certain embodiments, the nanoparticles are fed into an electrostatic spraying device at a flow rate and an atomization pressure, the flow rate is set to be 3-8ml/min, the atomization pressure of the electrostatic spraying device is 0.2-0.6MPa, the spraying distance is 10-20mm, the spraying time is 0.3-0.8min, and the coating thickness is 0.5-1 μm.
Wherein: the fumed silica is fed into a spraying device, and is loaded under the action of high-voltage direct current in the device to be sprayed onto the surface of the semi-molten liquid contact layer in an electric acceleration way. The particles repel each other during spraying and become more dispersed and more uniform. And compared with suspension plasma spraying, the method can effectively reduce adverse factors such as oxidization, phase change and the like.
Furthermore, nano particles are fed into the equipment at a certain flow rate and atomization pressure, and the paint atomization device is a negative electrode by utilizing the principle of like-pole repulsion and opposite-pole attraction, so that an electrostatic field is formed under the action of the two poles. Corona discharge occurs at the cathode, and the charged paint is sprayed out, and positively charged paint is uniformly coated on the surface along the electric line of force.
In certain embodiments, in step S4, the temperature of the cooling set is 25-45 ℃.
In some embodiments, the method further comprises a winding forming step after the film is subjected to secondary lamination, and before the film is subjected to winding forming, the corners of the film are subjected to cutting treatment.
The beneficial effects are that: in order to obtain higher mechanical property and better cell culture effect, the invention adopts a multilayer coextrusion casting extrusion process, and performs electrostatic spraying on the liquid contact layer of the membrane material to cover a layer of fumed silica on the surface of the membrane material, thus obtaining the higher cell culture effect through a large number of experiments. The multilayer co-extrusion bioreactor membrane material has better biocompatibility, higher gas barrier property and high bending resistance and puncture resistance.
Drawings
FIG. 1 is a schematic structural diagram of a multilayer coextruded bioreactor membrane in example 1.
Detailed Description
The present invention will be described in further detail with reference to the following embodiments.
Example 1
As shown in FIG. 1, the membrane material of the multilayer co-extrusion bioreactor comprises the following structures from outside to inside in sequence:
a protective layer 1, an adhesive layer 2, a gas barrier layer 3, an adhesive layer 4, a liquid contact layer 5 and a coating 6.
Example 2
The preparation method of the multilayer coextrusion bioreactor membrane material comprises the following steps:
d1, heating and melting extrusion of a film material through a multilayer coextrusion device, and controlling during melting extrusion: the preheating temperature of the multilayer coextrusion equipment is 120 ℃, and the heating time is 90min; the die temperature was 200 ℃; the temperature of the feed inlet is 80 ℃, so that particles are convenient to convey;
the membrane material sequentially comprises a protective layer, an adhesive layer, a gas barrier layer, an adhesive layer and a liquid contact layer from outside to inside;
the protective layer is composed of mixed resin of linear low-density polyethylene and metallocene polyethylene, the thickness of the protective layer is 50-80 mu m, the mass ratio of the linear low-density polyethylene is 60%, and the mass ratio of the metallocene polyethylene is 40%; the adhesive layer is made of ethylene-vinyl acetate copolymer, the thickness of the adhesive layer is 10-18 mu m, and the melt extrusion temperature is 160 ℃; the gas barrier layer is made of ethylene-vinyl alcohol copolymer, and the thickness of the gas barrier layer is 20-60 mu m; the liquid contact layer is made of metallocene polyethylene and linear low-density polyethylene, the thickness of the liquid contact layer is 150-250 mu m, the mass ratio of the metallocene polyethylene is 10%, and the mass ratio of the linear low-density polyethylene is 90%; and
conveying the film material to a stretching traction roller in a stretching system;
d2, performing thickness test on the extruded film, including the following steps:
stretching the film, obtaining infrared images, and testing the thickness of each edge;
d3, conveying the film material through a traction roller, performing primary cooling by a cooling roller, shaping, and controlling the cooling temperature of the first group of cooling rollers to be 60 ℃;
d4, carrying out secondary heating on the liquid contact layer through infrared radiation heating equipment, wherein the heating temperature is 120 ℃, forming a semi-molten state, and carrying out electrostatic spraying on nano particles on the liquid contact layer;
specifically, the nano particles are prepared by proportionally mixing fumed silica and a dispersing agent;
wherein: the particle size of the fumed silica is 0.02 μm; the dispersing agent is selected from polymethacrylic acid, and the mass ratio of the dispersing agent is controlled to be 0.8%.
Feeding the nano particles into electrostatic spraying equipment at a certain flow rate and atomization pressure, wherein the flow rate is set to be 3ml/min, the atomization pressure of the electrostatic spraying equipment is set to be 0.2MPa, the spraying distance is set to be 10mm, the spraying time is set to be 0.3min, and the thickness of a coating is set to be 0.5-1 mu m;
d5, performing secondary lamination on the film through a second group of cooling rollers, and controlling the cooling and shaping temperature to be 25 ℃;
and D6, performing a rolling forming step after the film is subjected to secondary lamination, and cutting corners of the film before the film is subjected to rolling forming.
Example 3
The preparation method of the multilayer coextrusion bioreactor membrane material comprises the following steps:
d1, heating and melting extrusion of a film material through a multilayer coextrusion device, and controlling during melting extrusion: the preheating temperature of the multilayer coextrusion equipment is 180 ℃, and the heating time is 60min; the die temperature was 220 ℃; the temperature of the feed inlet is 120 ℃, so that particles are convenient to convey;
the membrane material sequentially comprises a protective layer, an adhesive layer, a gas barrier layer, an adhesive layer and a liquid contact layer from outside to inside;
the protective layer is composed of mixed resin of linear low-density polyethylene and metallocene polyethylene, the thickness of the protective layer is 50-80 mu m, the mass ratio of the linear low-density polyethylene is 75%, and the mass ratio of the metallocene polyethylene is 25%; the adhesive layer is made of ethylene-vinyl acetate copolymer, the thickness of the adhesive layer is 10-18 mu m, and the melt extrusion temperature is 180 ℃; the gas barrier layer is made of ethylene-vinyl alcohol copolymer, and the thickness of the gas barrier layer is 20-60 mu m; the liquid contact layer is made of metallocene polyethylene and linear low-density polyethylene, the thickness of the liquid contact layer is 150-250 mu m, the mass ratio of the metallocene polyethylene is 25%, and the mass ratio of the linear low-density polyethylene is 75%; and
conveying the film material to a stretching traction roller in a stretching system;
d2, performing thickness test on the extruded film, including the following steps:
stretching the film, obtaining infrared images, and testing the thickness of each edge;
d3, conveying the film material through a traction roller, performing primary cooling by a cooling roller, shaping, and controlling the cooling temperature of the first group of cooling rollers to be 110 ℃;
d4, carrying out secondary heating on the liquid contact layer through infrared radiation heating equipment, wherein the heating temperature is 150 ℃, forming a semi-molten state, and carrying out electrostatic spraying on nano particles on the liquid contact layer;
specifically, the nano particles are prepared by proportionally mixing fumed silica and a dispersing agent;
wherein: the particle size of the fumed silica is 0.02 μm; the dispersing agent is selected from polymethacrylic acid, and the mass ratio of the dispersing agent is controlled to be 0.8%.
The nano particles are sent into electrostatic spraying equipment at a certain flow rate and atomization pressure, the flow rate is set to be 5ml/min, the atomization pressure of the electrostatic spraying equipment is set to be 0.4MPa, the spraying distance is set to be 15mm, the spraying time is set to be 0.5min, and the thickness of the coating is set to be 0.5-1 mu m.
D5, performing secondary lamination on the film through a second group of cooling rollers, and controlling the cooling and shaping temperature to be 35 ℃;
and D6, performing a rolling forming step after the film is subjected to secondary lamination, and cutting corners of the film before the film is subjected to rolling forming.
Example 4
The preparation method of the multilayer coextrusion bioreactor membrane material comprises the following steps:
d1, heating and melting extrusion of a film material through a multilayer coextrusion device, and controlling during melting extrusion: the preheating temperature of the multilayer coextrusion equipment is 240 ℃, and the heating time is 30min; the die temperature was 250 ℃; the temperature of the feed inlet is 150 ℃, so that particles are convenient to convey;
the membrane material sequentially comprises a protective layer, an adhesive layer, a gas barrier layer, an adhesive layer and a liquid contact layer from outside to inside;
the protective layer is composed of mixed resin of linear low-density polyethylene and metallocene polyethylene, the thickness of the protective layer is 50-80 mu m, the mass ratio of the linear low-density polyethylene is 90%, and the mass ratio of the metallocene polyethylene is 10%; the adhesive layer is made of ethylene-vinyl acetate copolymer, the thickness of the adhesive layer is 10-18 mu m, and the melt extrusion temperature is 200 ℃; the gas barrier layer is made of ethylene-vinyl alcohol copolymer, and the thickness of the gas barrier layer is 20-60 mu m; the liquid contact layer is made of metallocene polyethylene and linear low-density polyethylene, the thickness of the liquid contact layer is 150-250 mu m, the mass ratio of the metallocene polyethylene is 40%, and the mass ratio of the linear low-density polyethylene is 60%; and
conveying the film material to a stretching traction roller in a stretching system;
d2, performing thickness test on the extruded film, including the following steps:
stretching the film, obtaining infrared images, and testing the thickness of each edge;
d3, conveying the film material through a traction roller, performing preliminary cooling by a cooling roller, shaping, and controlling the cooling temperature of the first group of cooling rollers to be 150 ℃;
d4, carrying out secondary heating on the liquid contact layer through infrared radiation heating equipment, wherein the heating temperature is 180 ℃, forming a semi-molten state, and carrying out electrostatic spraying on nano particles on the liquid contact layer;
specifically, the nano particles are prepared by proportionally mixing fumed silica and a dispersing agent;
wherein: the particle size of the fumed silica is 0.02 μm; the dispersing agent is selected from polymethacrylic acid, and the mass ratio of the dispersing agent is controlled to be 0.8%.
The nano particles are sent into electrostatic spraying equipment at a certain flow rate and atomization pressure, the flow rate is set to be 8ml/min, the atomization pressure of the electrostatic spraying equipment is set to be 0.6MPa, the spraying distance is set to be 20mm, the spraying time is set to be 0.8min, and the thickness of the coating is set to be 0.5-1 mu m.
D5, performing secondary lamination on the film through a second group of cooling rollers, and controlling the cooling and shaping temperature to be 45 ℃;
and D6, performing a rolling forming step after the film is subjected to secondary lamination, and cutting corners of the film before the film is subjected to rolling forming.
In particular, instead of fumed silica, substances such as calcium phosphate (Ca 3 (PO 4 ) 2 ) Calcium carbonate (CaCO) 3 ) Calcium sulfate (CaSO) 4 ) Calcium silicate (CaSiO) 4 ) Etc. The preparation process of the particles for preparing the liquid contact layer and the preparation process of the multilayer co-extrusion bioreactor membrane material are the same by using the substances to replace fumed silica.
Comparative example 1
The preparation process of the multilayer co-extrusion bioreactor membrane material is the same as that of the embodiment 2, and only the preparation raw materials in the protective layer are changed into linear low-density polyethylene.
Comparative example 2
The preparation process of the multilayer co-extrusion bioreactor membrane material is the same as that of the embodiment 2, and only the preparation raw material in the protective layer is changed into metallocene polyethylene.
Comparative example 3
The preparation process of the multilayer coextrusion bioreactor membrane material is the same as that of the embodiment 2, and the step of carrying out electrostatic spraying on the liquid contact layer and applying fumed silica is only removed.
Performance testing
The tensile strength, transparency, oxygen transmittance and water vapor transmission amount of the process bag film material and the biocompatibility are detected, and the method specifically comprises the following steps:
A. the tensile strength of the film is tested according to ASTM D882, samples are made into strip shapes as required, the test is carried out at a speed of 25mm/min, 5 to 10 samples are prepared for each sample, and the average value is calculated;
B. the transparency of the film is tested according to ASTM D1003, a haze meter method is adopted, and samples are tested by standard adjustment for 40 hours under the environment of 23 ℃ plus or minus 2 ℃ and 50% plus or minus 10% humidity, wherein each group of 3 samples are tested;
C. the water vapor permeability of the membrane material is tested according to ASTM E96, a weighing method is adopted for testing, 3 samples are used in each group, and an average value is obtained;
D. the oxygen transmittance of the film material is tested according to ASTM D3985, the film is detected by adopting an electric quantity analysis method, and finally, the average value is obtained;
E. the multi-layer co-extrusion bioreactor membrane material is welded by an automatic cycle welding machine to prepare a disposable biotechnology bag with 5L specification, and is subjected to beta-ray radiation sterilization treatment. And (3) carrying out biocompatibility test on the process bag, culturing HEK293 cells, wherein the initial concentration of the cells is 10 ten thousand cells/ml, the culturing temperature is 36.5+/-0.5 ℃, the culturing time is 5-7 days, the stirring speed is 200rpm, and detecting the cell density after the culturing is finished.
1. The influence of different protective layers on the performance of the multilayer co-extrusion bioreactor membrane material is examined, and specific results are shown in table 1:
TABLE 1
As can be seen from Table 1, the different protective layers have a certain effect on the tensile strength, oxygen transmission, water vapor transmission, transparency and cell culture density of the multilayer coextruded bioreactor membranes.
The tensile strength, the transparency, the oxygen permeability and the cell culture effect of respectively adopting the mPE and the LLDPE as the protective layers are in accordance with the preparation requirements of the disposable bioreactor membrane material. However, when the mixture of mPE and LLDPE is used, both tensile strength and weld strength are significantly better than comparative examples 1 and 2; it is therefore preferred to use a blend of mPE and LLDPE as the protective layer.
2. The influence of different liquid contact layers on the membrane material of the multilayer co-extrusion bioreactor is examined, and the specific results are shown in table 2:
TABLE 2
As can be seen from Table 2, the different liquid contact layers have a certain influence on the tensile strength, oxygen transmission, water vapor transmission, transparency and cell culture density of the multilayer co-extruded bioreactor membrane material, and in particular have a remarkable influence on the cell culture effect.
When the liquid contact layer contains fumed silica, the prepared multilayer co-extrusion bioreactor membrane material has proper tensile strength, oxygen transmission amount, water vapor transmission amount and transparency, and the cell culture density is greatly improved, which is probably due to fumed silica (SiO 2 ) Has better biocompatibility. The thickness of the coating is controlled to be 0.5-1 μm during the spraying process, if SiO 2 Too high an addition level of (c) will affect physical properties.
To sum up: the invention provides a preparation method of a novel disposable multilayer co-extrusion bioreactor membrane material, which comprises a protective layer, an adhesive layer, a gas barrier layer, an adhesive layer and a liquid contact layer from outside to inside. The liquid contact layer adopts a secondary spraying technology, a film material is extruded through a multilayer co-extrusion device, the surface of the liquid contact layer is semi-molten after being heated by secondary radiation, a layer of fumed silica is sprayed on the liquid contact layer in an electrostatic mode, and then the liquid contact layer is pressed through a cold pressing roller. The preparation method is simple to operate, low in cost and capable of mass production. The disposable multilayer coextrusion bioreactor membrane material prepared by the method has higher mechanical property and better cell culture effect.
The above description is only of a preferred form of the invention, it being noted that it will be apparent to those skilled in the art that several variations and modifications can be made without departing from the inventive concept, which shall also be regarded as being within the scope of the invention.
Claims (10)
1. The preparation method of the multilayer coextrusion bioreactor membrane material is characterized by comprising the following steps of:
s1, heating and melting extrusion of a film material through a multilayer coextrusion device, and conveying the film material to a stretching traction roller in a stretching system;
s2, conveying the film material through a traction roller, performing preliminary cooling by a cooling roller, and shaping;
s3, carrying out secondary heating on the liquid contact layer through infrared radiation heating equipment to form a semi-molten state, and carrying out electrostatic spraying on the liquid contact layer with nano particles;
s4, performing secondary lamination on the film through a second group of cooling rollers.
2. The method for preparing a multilayer coextrusion bioreactor membrane material according to claim 1, wherein in the step S1, the preheating temperature of the multilayer coextrusion device is 120-240 ℃ and the heating time is 30-90min; the temperature of the die head is 200-250 ℃; the temperature of the feed inlet is 80-150 ℃, so that the particles can be conveniently conveyed.
3. The method for preparing a multilayer coextrusion bioreactor membrane according to claim 1, wherein in step S1, the membrane comprises a protective layer, an adhesive layer, a gas barrier layer, an adhesive layer and a liquid contact layer in sequence from outside to inside;
the protective layer is composed of mixed resin of linear low-density polyethylene and metallocene polyethylene, the thickness of the protective layer is 50-80 mu m, the mass ratio of the linear low-density polyethylene is 60-90%, and the mass ratio of the metallocene polyethylene is 10-40%; the adhesive layer is made of ethylene-vinyl acetate copolymer, the thickness of the adhesive layer is 10-18 mu m, and the melt extrusion temperature is 160-200 ℃; the gas barrier layer is made of ethylene-vinyl alcohol copolymer, and the thickness of the gas barrier layer is 20-60 mu m; the liquid contact layer is made of metallocene polyethylene and linear low-density polyethylene, the thickness of the liquid contact layer is 150-250 mu m, the mass ratio of the metallocene polyethylene is 10-40%, and the mass ratio of the linear low-density polyethylene is 60-90%.
4. The method for preparing a multilayer co-extruded bioreactor membrane according to claim 1, further comprising the step of performing a thickness test on the extruded membrane, comprising the steps of:
the film was stretched and an infrared image was obtained and the thickness of each edge was tested.
5. The method for producing a multilayer coextruded bioreactor film according to claim 1, characterized in that in step S2, the cooling temperature of the first set of cooling rolls is 60-150 ℃.
6. The method for preparing a multilayer coextrusion bioreactor film according to claim 1, wherein in step S3, the heating temperature is 120-180 ℃.
7. The method for preparing a multilayer coextrusion bioreactor membrane according to claim 1, wherein in step S3, nanoparticles are prepared by mixing fumed silica and a dispersing agent in proportion;
wherein: the particle size of the fumed silica is 0.02 μm; the dispersing agent is selected from polymethacrylic acid, and the mass ratio of the dispersing agent is controlled to be 0.8%.
8. The method for preparing the multilayer coextrusion bioreactor membrane material according to claim 7, wherein the nanoparticles are fed into an electrostatic spraying device at a certain flow rate and an atomization pressure, the flow rate is set to be 3-8ml/min, the atomization pressure of the electrostatic spraying device is 0.2-0.6MPa, the spraying distance is 10-20mm, the spraying time is 0.3-0.8min, and the coating thickness is 0.5-1 μm.
9. The method for preparing a multilayer coextrusion bioreactor film according to claim 1, wherein in step S4, the temperature for cooling and shaping is 25-45 ℃.
10. The method for preparing the membrane material of the multilayer coextrusion bioreactor according to claim 1, further comprising a winding and forming step after the second lamination, wherein before winding and forming the membrane, cutting off corners of the membrane is needed.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN117698246A (en) * | 2023-12-15 | 2024-03-15 | 上海亮黑科技有限公司 | Special membrane for biological cell culture and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN117698246A (en) * | 2023-12-15 | 2024-03-15 | 上海亮黑科技有限公司 | Special membrane for biological cell culture and preparation method thereof |
| CN117698246B (en) * | 2023-12-15 | 2024-06-18 | 上海亮黑科技有限公司 | Special membrane for biological cell culture and preparation method thereof |
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